Water → Cyclopropanemethanol, 2,2-difluoro-, 1-methanesulfonate

HRID 1026326

반응식

HRID 1026326 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]1([F:12])[CH2:9][CH:8]1[CH2:10][OH:11].C(N(CC)CC)C.O>C1COCC1>[CH3:1][S:2]([O:11][CH2:10][CH:8]1[CH2:9][C:7]1([F:12])[F:6])(=[O:4])=[O:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2761401(2,2-Difluorocyclopropyl)methanol

생성물 1

HCID 58198163Cyclopropanemethanol, 2,2-difluoro-, 1-methanesulfonate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methanesulfonyl chloride (1.43 mL) was added to a solution of (2,2-difluorocyclopropyl)methanol (1.00 g) and triethylamine (2.58 mL) in THF (10 mL) dropwise at 0° C. The mixture was stirred at room temperature overnight. Water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (1.47 g) as a colorless oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-8b19d6c282684771ab89f3e86b77613a
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729102B2

연결된 노트

불러오는 중…